CN103743853B - Rapid detection method of chemical components illegally added in Chinese patent medicine Xiaohuoluo pills - Google Patents
Rapid detection method of chemical components illegally added in Chinese patent medicine Xiaohuoluo pills Download PDFInfo
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- CN103743853B CN103743853B CN201410042641.3A CN201410042641A CN103743853B CN 103743853 B CN103743853 B CN 103743853B CN 201410042641 A CN201410042641 A CN 201410042641A CN 103743853 B CN103743853 B CN 103743853B
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Abstract
The invention relates to a rapid detection method of chemical components illegally added in Chinese patent medicine Xiaohuoluo pills. The method comprises the following steps: firstly, preparing a reference solution and a sample solution; respectively suctioning the reference solution and the sample solution; dripping on the same silica gel thin layer plate; adding a developing agent for ascending development; taking out and drying in the air; placing below an ultraviolet lamp and observing thin-layer chromatogram; spraying sulfuric acid-ethanol solution; placing in an oven and heating at a constant temperature until spots on the thin layer plate are clear; respectively placing below a fluorescent lamp and the ultraviolet lamp and observing thin-layer chromatogram; and determining that the sample result is positive if fluorescence quenching spots, fluorescence spots or spots with the same color occur at the same time at a point with a retardation factor value same as that of the reference. Obviously, the method provided by the invention is simple to operate, rapid, and cost-effective, not only solves the problem of false positive interference, but also avoids expensive cost and plenty of time consumed by the conventional infrared spectroscopy, HPLC-MS and the like, thereby making it possible to effectively monitor whether chemical components are illegally added in the Xiaohuoluo pills.
Description
Technical field
The present invention relates to traditional Chinese medicine quality detection field, be specifically related to the illegal method for quick adding chemical substance in a kind of Chinese patent drug Small Meridian-Activating Pill.
Background technology
Small Meridian-Activating Pill is by arisaema cum bile, aconiti preparata,radix, wild aconite root, earthworm, frankincense (system), myrrh (system) Chinese medicine preparation that forms of the totally 6 taste prepared slices of Chinese crude drugs.Primary efficacy is expelling wind and clearing away cold, dehumidifying of reducing phlegm, promoting blood circulation and stopping pain.Sick for the numbness caused by wind-cold damp pathogen impatency, phlegm stagnation in collateral, disease sees limbs joint pain, or crymodynia, or shouting pain, or pain night very, joint joint stuffiness, numbness contracture.Its preparation method is that arisaema cum bile, aconiti preparata,radix, wild aconite root, earthworm, frankincense (system), myrrh (system) are ground into fine powder respectively, sieves, and mixing, every 100g fine powder adds refined honey 120 ~ 130g and makes large honeyed bolus.This Chinese medicine preparation complicated component, the clinical bi Zheng such as pain in the back, skelagia, cervicodynia, brachialgia being used for the treatment of rheumatic arthritis, rheumatoid arthritis and caused by hyperosteogeny, sciatica, duodenal stasis etc.Belong to Anti-rheumatism Chinese patent drugs.In order to pursue economic interests, some lawless persons illegal interpolation in Small Meridian-Activating Pill has antipyretic, anti-inflammatory, analgesic effect cheap chemical substance, to reach effect effective fast.And patient after too much these chemical substances of absorption, can cause great harm to health in unwitting situation.
In Anti-rheumatism Chinese patent drugs, illegal chemical substance of adding mainly contains two large classes: antipyretic-antalgic class and glucocorticoids.At present, the illegal method of adding chemical substance in Anti-rheumatism Chinese patent drugs that detects is the universal method not limiting the concrete kind of Chinese patent drug.This universal method relates to all Anti-rheumatism Chinese patent drugs, and scope is wide, but Anti-rheumatism Chinese patent drugs is of a great variety, and the prescription of each Chinese patent drug is all different, very easily produce vacation " positive " interference, cannot result of determination clearly, therefore universal method only can accomplish scalping.And due to the interference of false " positive ", the chemical substance detected is only limitted in antipyretic-antalgic class or glucocorticoids limited several.As " the detection method research about undeclared prescription drugs in antirheumatic Chinese medicine preparation " (Asia-Pacific traditional medicine .2010.6(6) such as Zhang He: 31-32) first adopt thin-layered chromatography to carry out scalping, then must infrared spectrum or high performance liquid chromatography be adopted to verify positive wherein further again.But due to infrared spectrometer, HPLC-MS, GC-MS expensive equipment, and must be manipulated by technical professional, maintenance cost is also high, the object that rapid screening reaches monitoring cannot be realized.Obviously, build for interpolation number of chemical material illegal in Small Meridian-Activating Pill the method carrying out rapid screening to be completely very important.Therefore, in order to make the illegal illegal activities adding chemical substance in Small Meridian-Activating Pill effectively be controlled, ensureing that the people is safe and effective for medication, needing badly and setting up the illegal quick screening method adding chemical substance in Small Meridian-Activating Pill.
Summary of the invention
The object of this invention is to provide the illegal method for quick adding chemical substance in a kind of Chinese patent drug Small Meridian-Activating Pill, to overcome the deficiencies in the prior art.
Another object of the present invention gets rid of Small Meridian-Activating Pill and illegal vacation " positive " interference adding chemical substance, realizes the rapid screening of multiple illegal interpolation chemical substance, reach the universal feasible of monitoring.
Small Meridian-Activating Pill is a Chinese medicine preparation, although prescription flavour of a drug are few, chemical composition is very complicated, illegally adds chemical substance in addition, very easily occurs that vacation " positive " is disturbed during mensuration.Usual vacation " positive " interference must adopt infrared spectrometer, HPLC-MS, GC-MS carry out composition confirmation.Research finds, because 10 kinds of chemical substances of examination required in Small Meridian-Activating Pill all have the character being dissolved in methyl alcohol, and methyl alcohol is low to the refined honey solubleness in large honeyed bolus, therefore utilizes this character, selects methyl alcohol as Extraction solvent.Consider that Small Meridian-Activating Pill is large honeyed bolus, if do not disperseed, this Extraction solvent cannot penetrate in sample, can not fully extract chemical substance to be measured.Therefore get Small Meridian-Activating Pill one ball (3g), after shredding, add zeyssatite grinding, large honeyed bolus fully can be disperseed.Add methyl alcohol again, sample is all soaked, and adopt ultrasonic process, effectively these 10 kinds of materials are extracted.Both can avoid the stripping of refined honey in Small Meridian-Activating Pill, be convenient to point sample, other compositions in Small Meridian-Activating Pill can have been greatly reduced again to the interference measured.Again because of the illegal difference of chemical substance on thin layer plate in adsorptive power of adding, then go out in Chinese patent drug Small Meridian-Activating Pill whether illegally with the addition of the chemical substance that 10 kinds are divided into 2 groups with developping agent examination respectively.
Quick screening method of the present invention is as follows
(1) preparation of reference substance solution: get prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and each 10mg of hydrocortisone acetate reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution A; Separately get paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and each 10mg of phenylbutazone reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution B.
(2) preparation of need testing solution: get Small Meridian-Activating Pill 3g, shred, adds zeyssatite 2g, grinds well, add methyl alcohol, ultrasonic process, filters, gets filtrate as need testing solution.
(3) examination mensuration is carried out: draw reference substance solution A1 μ l respectively, need testing solution 5 μ l, puts in same silica G F
254on thin layer plate, with developping agent I ascending development, take out, dry, observe thin-layer chromatography under putting ultraviolet lamp (wavelength 254nm), and then spray 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then put observed under daylight thin-layer chromatography.In the chromatogram of above-mentioned two kinds of view modes, Rf value place identical with reference substance occurs if any the fluorescent quenching spot of same color or spot simultaneously, then can judge that sample result is as the positive.
The another reference substance solution B1 of absorption respectively μ l, need testing solution 5 μ l, puts in same silica G F
254on thin layer plate, with developping agent II ascending development, take out, dry, thin-layer chromatography is observed under putting ultraviolet lamp (wavelength 254nm), and then spray is with 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then observes thin-layer chromatography under putting daylight and ultraviolet lamp (wavelength 365nm) respectively.In the chromatogram of above-mentioned three kinds of view modes, Rf value place identical with reference substance occurs if any the fluorescent quenching spot of same color, fluorescence spot or spot simultaneously, then can judge that sample result is as the positive.
Above-mentioned developping agent I is methenyl choloride-acetone-methanol-strong ammonia solution=18: 6: 2: 0.1(volume ratio).
Above-mentioned developping agent II is n-hexane-ethyl acetate-methyl alcohol=32: 18: 5(volume ratio).
The condition of above-mentioned ultrasonic process is 30 minutes, power 250W, frequency 50kHz.
The method judges from being prepared into of reference substance solution sample result, and overall process only needs 1 hour, and can at same silica G F
254the product of the multiple producer of examination on thin layer plate.Obviously, the inventive method is easy and simple to handle, fast, cost is low, both the problem that vacation " positive " that Small Meridian-Activating Pill patent medicine causes because of complicated component is disturbed had been solved, it also avoid and adopt infrared spectrum, HPLC-MS, GC-MS measure the expensive expense and plenty of time that produce, are therefore whether illegally add chemical substance in effective monitoring Chinese patent drug Small Meridian-Activating Pill to become possibility.
Accompanying drawing explanation
Fig. 1: Small Meridian-Activating Pill of the present invention and prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, the TLC chromatogram of hydrocortisone acetate under developping agent I and ultraviolet lamp (wavelength 254nm) condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution A(spot a: prednisolone; Spot b: hydrocortisone; Spot c: metacortandracin; Spot d: Triamcinolone acetonide; Spot e: hydrocortisone acetate).
Fig. 2: Small Meridian-Activating Pill of the present invention and prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, the TLC chromatogram of hydrocortisone acetate under developping agent I and sunshine condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution A(spot a: prednisolone; Spot b: hydrocortisone; Spot c: metacortandracin; Spot d: Triamcinolone acetonide; Spot e: hydrocortisone acetate).
The need testing solution of the Small Meridian-Activating Pill negative sample in above-mentioned Fig. 1, Fig. 2 is not containing the need testing solution that the Small Meridian-Activating Pill sample of prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, hydrocortisone acetate is prepared according to the preparation method of need testing solution.The need testing solution of Small Meridian-Activating Pill positive is the need testing solution that the Small Meridian-Activating Pill sample containing prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, hydrocortisone acetate is prepared according to the preparation method of need testing solution.
Fig. 3: Small Meridian-Activating Pill of the present invention and paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate, the TLC chromatogram of phenylbutazone under developping agent II and ultraviolet lamp (wavelength 254nm) condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution B(spot a: paracetamol; Spot b: dexamethasone; Spot c: cortisone acetate; Spot d: triamcinolone acetonide acetate; Spot e: phenylbutazone).
Fig. 4: Small Meridian-Activating Pill of the present invention and paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate, the TLC chromatogram of phenylbutazone under developping agent II and ultraviolet lamp (wavelength 365nm) condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution B(spot b: dexamethasone; Spot c: cortisone acetate; Spot d: triamcinolone acetonide acetate; Spot e: phenylbutazone).
Fig. 5: Small Meridian-Activating Pill of the present invention and paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate, the TLC chromatogram of phenylbutazone under developping agent II and sunshine condition; Wherein, 1: the need testing solution of Small Meridian-Activating Pill negative sample; 2: the need testing solution of Small Meridian-Activating Pill positive; 3: reference substance solution B(spot b: dexamethasone; Spot c: cortisone acetate; Spot d: triamcinolone acetonide acetate; Spot e: phenylbutazone).
The need testing solution of the Small Meridian-Activating Pill negative sample in above-mentioned Fig. 3, Fig. 4, Fig. 5 is not containing the need testing solution that the Small Meridian-Activating Pill sample of paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate, phenylbutazone is prepared according to the preparation method of need testing solution.The need testing solution of Small Meridian-Activating Pill positive is the need testing solution that the Small Meridian-Activating Pill sample containing paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate, phenylbutazone is prepared according to the preparation method of need testing solution.
Embodiment
Provide detailed embodiment below.
The present invention adopts: instrument and reagent: Sartoris BP211D electronic balance, AUTO SCIENCEAS10200BT type ultrasonic cleaner, P/G2007 type constant temperature oven, thin layer plate: silica G F
254thin layer plate (German MERCK lot number: HX929689 specification: 20 × 20cm), it is pure that reagent is analysis, prednisolone reference substance (lot number: 100153-201004), hydrocortisone reference substance (lot number: 100152-200206), metacortandracin reference substance (lot number: 100199-201002), Triamcinolone acetonide reference substance (lot number: 100055-201103), hydrocortisone acetate reference substance (lot number: 100013-200607), paracetamol reference substance (lot number: 100018-200408), dexamethasone reference substance (lot number: 100129-201105), cortisone acetate reference substance (lot number: 100123-200303), triamcinolone acetonide acetate reference substance (lot number: 100125-201105), phenylbutazone reference substance (lot number: 100481-200601), above reference substance provides by National Institute for Food and Drugs Control, Small Meridian-Activating Pill (indicates lot number: 130110,20130715,130401,120801,20121201,120012,2111105).
Chromatographic condition: developping agent I: methenyl choloride-acetone-methanol-strong ammonia solution=18: 6: 2: 0.1 (volume ratios); Developping agent II: n-hexane-ethyl acetate-methyl alcohol=32: 18: 5 (volume ratios); Unfolding condition: temperature: 23 DEG C; Relative humidity: 59%; Exhibition distance: 10cm.
The preparation of reference substance solution: get prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and each 10mg of hydrocortisone acetate reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution A; Separately get paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and each 10mg of phenylbutazone reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution B.
The preparation of need testing solution: get Small Meridian-Activating Pill finished product 3g, shred, add zeyssatite 2g, grind well, add methyl alcohol 10ml, carry out ultrasonic process, filters, gets filtrate as need testing solution.
Above-mentioned ultrasonic treatment conditions are 30 minutes, power 250W, frequency 50kHz.
Carry out examination mensuration: draw reference substance solution A1 μ l respectively, need testing solution 5 μ l, puts in same silica G F
254on thin layer plate, with developping agent I ascending development, take out, dry, observe thin-layer chromatography under putting ultraviolet lamp (wavelength 254nm), and then spray 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then put observed under daylight thin-layer chromatography.In the chromatogram of above-mentioned two kinds of view modes, Rf value place identical with reference substance occurs if any the fluorescent quenching spot of same color or spot simultaneously, then can judge that sample result is as the positive.Having detected 5 kinds of chemical substances is prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and hydrocortisone acetate.Corresponding chromatogram as shown in Figure 1, Figure 2.
The another reference substance solution B1 of absorption respectively μ l, need testing solution 5 μ l, puts in same silica G F
254on thin layer plate, with developping agent II ascending development, take out, dry, thin-layer chromatography is observed under putting ultraviolet lamp (wavelength 254nm), and then spray is with 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then observes thin-layer chromatography under putting daylight and ultraviolet lamp (wavelength 365nm) respectively.In the chromatogram of above-mentioned three kinds of view modes, Rf value place identical with reference substance occurs if any the fluorescent quenching spot of same color, fluorescence spot or spot simultaneously, then can judge that sample result is as the positive.Having detected again 5 kinds of chemical substances is paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and phenylbutazone.Corresponding chromatogram is as Fig. 3, Fig. 4, Fig. 5.
Result shows, 2 groups of mixing reference substance good separations, and all the components of Small Meridian-Activating Pill self is noiseless to mensuration, and namely at reference substance identical Rf value place, noiseless composition exists test sample.
To sum up, the thin-layered chromatography that the present invention sets up can detect in Chinese patent drug Small Meridian-Activating Pill whether illegally with the addition of these 10 kinds of chemical substances of prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide, hydrocortisone acetate, paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and phenylbutazone fast, have easy and simple to handle, fast, the feature of low cost, can as the universal method of Small Meridian-Activating Pill Quality of Chinese Traditional Proprietary Medicine monitoring.
Claims (6)
1. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill, is characterized in that preparing each reference substance solution (1) and need testing solution (2) first respectively, then carries out examination mensuration (3):
(1) preparation of reference substance solution: get prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and each 10mg of hydrocortisone acetate reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution A; Separately get paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and each 10mg of phenylbutazone reference substance respectively, dissolve with methyl alcohol 10ml, make reference substance solution B;
(2) preparation of need testing solution: get Small Meridian-Activating Pill one ball, shred, add zeyssatite, grind well, add methyl alcohol, ultrasonic process, filters, gets filtrate as need testing solution;
(3) examination mensuration is carried out: draw reference substance solution A respectively, need testing solution, point sample is in same silica G F
254on thin layer plate, using methenyl choloride-acetone-methanol-strong ammonia solution as developping agent ascending development, take out, dry, thin-layer chromatography is observed under putting ultraviolet lamp 254nm, spray again with 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then puts observed under daylight thin-layer chromatography; If in the chromatogram of above-mentioned two kinds of view modes, Rf value place identical with reference substance has the fluorescent quenching spot of same color or spot to occur simultaneously, then can judge that sample result is as the positive, having detected 5 kinds of chemical substances is prednisolone, hydrocortisone, metacortandracin, Triamcinolone acetonide and hydrocortisone acetate;
Separately, draw reference substance solution B respectively, need testing solution, point sample is in same silica G F
254on thin layer plate, using n-hexane-ethyl acetate-methyl alcohol as developping agent ascending development, take out, dry, thin-layer chromatography is observed under putting ultraviolet lamp 254nm, spray again with 10% ethanol solution of sulfuric acid, and it is clear to the spot development on thin layer plate to be placed in 105 DEG C of baking oven heated at constant temperature, then observes thin-layer chromatography under putting daylight and ultraviolet lamp 365nm respectively; If in the chromatogram of above-mentioned three kinds of view modes, Rf value place identical with reference substance has the fluorescent quenching spot of same color, fluorescence spot or spot to occur simultaneously, then can judge that sample result is as the positive, having detected again 5 kinds of chemical substances is paracetamol, dexamethasone, cortisone acetate, triamcinolone acetonide acetate and phenylbutazone; The volume ratio of above-mentioned developping agent methenyl choloride-acetone-methanol-strong ammonia solution is 18: 6: 2: 0.1; The volume ratio of above-mentioned developping agent n-hexane-ethyl acetate-methyl alcohol is 32: 18: 5.
2. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill as claimed in claim 1, is characterized in that above-mentioned zeyssatite weight is 2g.
3. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill as claimed in claim 1, is characterized in that the methyl alcohol volume in the preparation of above-mentioned (2) need testing solution is 10ml.
4. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill as claimed in claim 1, is characterized in that the point sample volume of above-mentioned each reference substance solution is 1 μ l.
5. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill as claimed in claim 1, is characterized in that the point sample volume of above-mentioned need testing solution is 5 μ l.
6. the illegal method for quick adding chemical substance in Chinese patent drug Small Meridian-Activating Pill as claimed in claim 1, is characterized in that the condition of above-mentioned ultrasonic process is 30 minutes, power 250W, frequency 50kHz.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1785166A (en) * | 2005-11-10 | 2006-06-14 | 贵州和仁堂药业有限公司 | Method for quality control of infantile amfenac alkylamine |
| CN1813770A (en) * | 2005-11-21 | 2006-08-09 | 咸阳步长医药科技发展有限公司 | Gel of triamcinolone acetonide and econazole nitrate, its preparing and quality control method |
| CN101762673A (en) * | 2009-12-09 | 2010-06-30 | 中国人民武装警察部队药品仪器检验所 | Method for detection of illegally added chemical in traditional Chinese medicine preparation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040033273A1 (en) * | 2001-02-14 | 2004-02-19 | Ayurcore, Inc. | Withasol and methods of use |
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Patent Citations (3)
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|---|---|---|---|---|
| CN1785166A (en) * | 2005-11-10 | 2006-06-14 | 贵州和仁堂药业有限公司 | Method for quality control of infantile amfenac alkylamine |
| CN1813770A (en) * | 2005-11-21 | 2006-08-09 | 咸阳步长医药科技发展有限公司 | Gel of triamcinolone acetonide and econazole nitrate, its preparing and quality control method |
| CN101762673A (en) * | 2009-12-09 | 2010-06-30 | 中国人民武装警察部队药品仪器检验所 | Method for detection of illegally added chemical in traditional Chinese medicine preparation |
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| Development of a high-performance thin-layer chromatographic method for the multi-screening analysis of corticosteroids;K E Vanoosthuyze et al;《Analytica Chimica Acta》;19931231;第275卷;177-182 * |
| 中药制剂中非法掺入化学药物成分的测定;刘起中 等;《中国药师》;20070831;第10卷(第8期);735-737 * |
| 薄层色谱法快速检测中成药中的激素类化合物;矫筱蔓 等;《华西药学杂志》;20100531;第25卷(第5期);595-597 * |
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